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1、南京航空航天大学硕士学位论文 I 摘 要 本文以有序介孔碳为载体，采用微波氧化、浸渍等方法在介孔碳上负载NiO，制备高比电容且循环性能稳定的超级电容器电极材料，以实现材料结构和性能之间的合理平衡。 首先以介孔氧化硅 SBA- 15 为模板合成有序介孔碳 CMK- 3，尝试采用微波氧化法对 CMK- 3 负载 NiO 以改善介孔碳的电容性能， 并与浸渍法进行对比。ICP 测试显示微波氧化法具有快速、均匀且负载率高的优势。采用该负载方法所得复合电极材料的比电容已达 295.9 F/g，高于浸渍法负载的 252.6 F/g。 又采用软模板法，以 F127 为模板剂，可溶酚醛树脂前驱体为碳源制备了有序
2、介孔碳 C- FDU- 15，采用微波氧化法负载不同量的 NiO。XPS 定性测试揭示：在微波辐射作用下，Ni2+转化为单质 Ni 和 Ni(OH)2的混合体，经空气煅烧均转化为 NiO，从而得到 NiO/C 复合电极材料。考察负载量的变化对介孔碳结构性能及电化学性能的影响，得出最佳负载量下，NiO/C 的比电容可达 407 F/g，增加 34.3%。 还尝试在合成 C- FDU- 15 的过程中加入镍盐，经空气煅烧转变为 NiO/C 复合电极材料。实验结果表明 NiO 负载量最佳时，介孔碳 C- FDU- 15 的比容量由307.4 F/g 提高到 444.1 F/g，增加 44.5%，其充
3、放电循环稳定性也得到了极大的提高。 本文还简化了介孔碳球的合成路线，尝试以未经烧结的介孔 SiO2球为模板，制备单分散性的有序介孔碳球。该方法得到的碳球比表面积大、粒径均匀，孔径在 24 nm 范围内可调， 同时考察不同合成温度以及硅酸盐/表面活性剂在水溶液中的浓度对碳球结构的影响。采用微波氧化法在碳球上定量负载 NiO后，其比电容及循环稳定性都得到了很大的提高。 关键词：NiO/C 复合电极材料，CMK- 3，C- FDU- 15，介孔碳球，微波氧化法 超级电容器 NiO/介孔碳复合电极材料的制备及其性能研究 II Abstract A series of ordered mesoporou
4、s carbons were used as carrier and NiO was supported on the carbons by microwave- oxidation and impregnation method. In order to achieve reasonable balance between structure and performance of material, NiO/C composite electrode material for supercapacitor with high specific capacitance and steady c
5、ycle capability was received. Microwave- oxidation method was firstly introduced to support NiO on CMK- 3 synthesized by SBA- 15 template for improving capacitance performance of mesoporous carbons and then contrasted to impregnation method. ICP test showed microwave- oxidation method had advantage
6、of speediness, uniformity and high supporting efficiency. The specific capacitance was improved to 295.9 F/g, which was much more than 252.6 F/g attained by impregnation method. Ordered mesoporous carbon C- FDU- 15 derived from the co- assembly of F127 and resol had been successfully synthesized by
7、soft template method, and then NiO was supported on C- FDU- 15 using microwave- oxidation method. XPS test proved that Ni2+ was transformed to mixture of Ni and Ni(OH)2 under microwave radiation, and then translated into NiO by air calcination. The effect of NiO content on structure and electrochemi
8、cal performance of ordered mesoporous carbon was investigated. The specific capacitance of NiO/C reached to 407 F/g with an increase of 34.3 % under proper NiO content. We also tried to add nickel salt in the preparation process of C- FDU- 15 and the nickel salt was translated to NiO after air calci
9、nation. Experiment results indicated that the specific capacitance of C- FDU- 15 was increased from 307.4 F/g to 444.1 F/g and the steady cycle capability of charge- discharge was greatly improved when the NiO content was appropriate. Monodisperse ordered mesoporous carbon spheres were synthesized b
10、y non- calcined SiO2 spheres as template for predigesting the synthetical course. The effect of reactive temperature and silicate/surfactant concentration on the structure of carbon spheres was investigated. Ordered mesoporous carbon spheres could then be obtained with high specific surface area, un
11、iform particle size and pore diameter 南京航空航天大学硕士学位论文 III of 24 nm. The specific capacitance and cycle capability were greatly improved after supporting quantitative NiO on carbon spheres by microwave- oxidation method. Key Words: NiO/C composite electrode material, CMK- 3, C- FDU- 15, mesoporous car
12、bon spheres, microwave- oxidation method 南京航空航天大学硕士学位论文 VII 图表清单 图清单 图 2.1 CMK- 3 负载 NiO 前后的小角 XRD图谱 .16 图 2.2 NiO/CMK- 3- E 及 NiO/CMK- 3- M 与 NiO 的 XRD 对照图谱.16 图 2.3 CMK- 3 负载 NiO 前后的 N2吸脱附等温曲线.17 图 2.4 CMK- 3 负载 NiO 前后的孔径分布曲线.18 图 2.5 a.CMK- 3, b.NiO/CMK- 3- E 及 c.NiO/CMK- 3- M 的 TEM 图.19 图 2.6 CM
13、K- 3 负载 NiO 前后的循环伏安曲线，扫描速率：5mV/s.20 图 2.7 NiO/CMK- 3- M 样品在不同扫描速率下的循环伏安曲线 .20 图 2.8 CMK- 3 负载 NiO 前后比容量随扫描速率的变化关系.21 图 2.9 CMK- 3 负载 NiO 前后的恒流充放电曲线.22 图 3.1 a.未煅烧样品及 b.0.02NiO/C- M 的 XPS 图谱 .29 图 3.2 C- FDU- 15 微波负载 NiO 前后的小角 XRD 图谱 .30 图 3.3 C- FDU- 15 微波负载 NiO 样品与 NiO 的大角 XRD 对照图谱 .31 图 3.4 C- FDU
14、- 15 微波负载 NiO 前后的 a.N2吸脱附等温曲线及 b.孔径分布曲线.32 图 3.5 a.C- FDU- 15, b.0.02NiO/C- M 及 c.0.04NiO/C- M 的 TEM 图 .34 图 3.6 a.C- FDU- 15, b.0.01NiO/C- M, c.0.02NiO/C- M 及 d.0.04NiO/C- M 的循环伏安图，扫描速率：5 mV/s.34 图 3.7 0.02NiO/C- M 在不同扫描速率下的循环伏安曲线图 .35 图 3.8 扫描速率对 C- FDU- 15 微波负载 NiO 前后的比电容的影响.36 图 3.9 C- FDU- 15 微波负载 NiO 前后的充放电曲线.37 图 3.10 C- FDU- 15 原位负载 NiO 前后的小角 XRD 图谱 .
